反应详情

温度

80 °C

To a solution of 1.07 g of 1-[6-(2,5-dimethylpyrrol-1-yl)pyridin-3-yl]propan-1-ol in 20 mL of ethanol heated to 80° C. is added a solution of 1.94 g of hydroxylamine hydrochloride in 1.6 mL of water, and the mixture is stirred for 24 hours at 80° C. After cooling to room temperature, the reaction medium is filtered and concentrated to dryness. The residue is purified by flash chromatography on a column of 100 g of silica, eluting with 400 mL of dichloromethane, then with 300 mL of ethyl acetate and then with a 95/5 mixture of dichloromethane and methanol. The fractions containing the expected product are combined and concentrated under vacuum to give 0.186 g of 2-amino-5-(1-ethoxypropyl)pyridine in the form of a brown oil.

1. temperatureAfter cooling to room temperature
2. filtrationthe reaction medium is filtered
3. concentrationconcentrated to dryness
4. customThe residue is purified by flash chromatography on a column of 100 g of silica
5. washeluting with 400 mL of dichloromethane
6. additionwith 300 mL of ethyl acetate and then with a 95/5 mixture of dichloromethane and methanol
7. additionThe fractions containing the expected product
8. concentrationconcentrated under vacuum